반응 #47092

ord-95be94d797e54a1cbb6ae47686dc6060

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과filtered through Celite
  2. 2
    기타the filtrate is evaporated
  3. 3
    workup.DISTILLATIONdistilled at

실험 절차

To a solution of cyclohexylmethanol (1.23 mL, 10.0 mmol) in dichloromethane (30 mL) is added rhodium (II) acetate dimer (11 mg) followed by ethyl diazoacetate (1.05 mL, 10.0 mmol). The reaction mixture is stirred at RT for 30 min. To the reaction mixture is added MeOH, and the reaction mixture is rotary evaporated, and the residue dissolved in Et2O, filtered through Celite, and the filtrate is evaporated and the residue is vacuum distilled at to give 2.02 g of the product 419. 1H NMR (CDCl3) δ 4.22 (q, 2 H), 4.05 (s, 2 H), 3.33 (d, 2 H), 1.8-1.5 (m, 7 H), 1.4-1.1 (m, 5 H), 1.1-0.9 (m, 2 H); MS: m/z 200 (M++1).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741493B2uspto-grants-2010_06